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CN116064189B - Diamond cutting fluid for silicon carbide wafer and preparation method thereof - Google Patents

Diamond cutting fluid for silicon carbide wafer and preparation method thereof Download PDF

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CN116064189B
CN116064189B CN202211594625.6A CN202211594625A CN116064189B CN 116064189 B CN116064189 B CN 116064189B CN 202211594625 A CN202211594625 A CN 202211594625A CN 116064189 B CN116064189 B CN 116064189B
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diamond
cutting fluid
silicon carbide
oil
solution
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CN116064189A (en
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刘丹丹
付存
赵亚雯
任欢欢
王森
汪静
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Henan Union Precision Material Co ltd
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    • G01N11/00Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
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    • C10M2209/103Polyethers, i.e. containing di- or higher polyoxyalkylene groups
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Abstract

The invention discloses a diamond cutting fluid for a silicon carbide wafer and a preparation method thereof, wherein the diamond cutting fluid comprises the following raw materials in percentage by weight: 8-20% of diamond powder, 0.5-2.5% of dispersing agent, 2-6% of surfactant, 10-40% of thixotrope solution and 31.5-79.5% of base oil; wherein, the thixotrope solution comprises the following raw materials: 85-97% of vegetable oil, 2-10% of aluminum stearate and 1-5% of oil anti-aging agent T501. The diamond cutting fluid is efficient and easy to clean, has a simple production mode and is easy to produce in mass; in addition, the method for detecting the yield value of the diamond cutting fluid can shorten the judging time of the suspension stability in the formula research and development process.

Description

Diamond cutting fluid for silicon carbide wafer and preparation method thereof
Technical Field
The invention relates to the technical field of silicon carbide cutting auxiliary materials, in particular to diamond cutting fluid for silicon carbide wafers and a preparation method thereof.
Background
Silicon carbide single crystal materials are representative of third-generation semiconductor materials, and have wide application fields and wide application prospects by virtue of excellent properties. Depending on the use of the device, a silicon carbide single crystal polished wafer is required to have high surface quality: smooth surface, low surface roughness, no defect and no damage, and has excellent TTV, warp and other surface parameters. The processing quality and precision of the silicon carbide material directly influence the performance of the device. However, the hardness of the silicon carbide material is large and is only about 0.5 lower than that of diamond; the material has high chemical stability and hardly reacts with any strong acid or strong alkali, so the material is in the current situation of high processing difficulty.
For the processing technology of silicon carbide materials, crystal cutting is a very critical link, and plays a decisive role in wafer quality. At present, the common wafer cutting in the market comprises diamond wire cutting, oil sand wire cutting and the like, the saw kerf loss of the diamond wire cutting is larger than that of the oil sand wire, the cutting precision is lower than that of the oil sand wire, and the problem of higher cost of a single silicon carbide wafer is considered, so that the cutting of the silicon carbide wafer in the market is still mainly carried out by the oil sand wire.
Common problems of the wafer after being cut by the wire cutting liquid in the market at present mainly comprise: TTV and WARP values do not meet the requirements, line marks, etc. The system containing inorganic suspending agents such as organic modified bentonite in the linear cutting fluid is difficult to clean in the later period, abrasive materials are easily accumulated in a pipeline after the machine is stopped, waste residues are formed in the later period, and the processing precision and the cutting life are affected; the cutting fluid system without inorganic suspending agent has the common problems of low system viscosity, poor suspension stability, easy sedimentation and delamination, poor adhesion effect of abrasive materials on steel wires, difficult cleaning and the like, and influences the processing efficiency.
Disclosure of Invention
In order to solve the problems, the invention provides a diamond cutting fluid for a silicon carbide wafer and a preparation method thereof, the diamond cutting fluid is efficient and easy to clean, the diamond cutting fluid consists of diamond cutting powder controlled by fine treatment and a uniform and stable carrier, wherein the carrier of the cutting fluid consists of base oil, thixotrope solution, a dispersing agent, a surfactant, an oil product anti-aging agent and the like, and the silicon carbide wafer can be used for multi-line cutting after the substances are uniformly mixed by a certain method. In addition, the method for detecting the yield value of the diamond cutting fluid is found to shorten the judging time of the suspension stability in the formula research and development process and accelerate the formula research and development progress.
The invention is realized by the following technical scheme:
the diamond cutting fluid for the silicon carbide wafer comprises the following raw materials in percentage by weight: 8-20% of diamond powder
0.5 To 2.5 percent of dispersing agent
2-6% Of surfactant
10-40% Of thixotrope solution
31.5 To 79.5 percent of base oil;
wherein, the thixotrope solution comprises the following raw materials:
85-97% of vegetable oil
2-10% Of aluminum stearate and 1-5% of oil product anti-aging agent T501;
Wherein the content of the aluminum stearate is not less than 99 percent; the oil anti-aging agent T501 is an oil additive T501 (the main component is 2, 6-di-tert-butyl p-methylphenol).
Preferably, the diamond powder comprises one or more of single crystal diamond, polycrystalline diamond and granular diamond, and the average grain diameter is 0.5-40um.
Preferably, the dispersant is DISPERBYK-2157, DISPER BYK-180, DISPER BYK-110,
One or more of DISPERBYK-P104S.
Preferably, the surfactant is one or more of tallow amine polyoxyethylene (5) ether, oleyl alcohol polyoxyethylene ether, dodecyl alcohol polyoxyethylene (3) ether, oleyl amine polyoxyethylene (2) ether and oleic acid triglyceride.
Preferably, the base oil is one or more of C10-C30 linear alkane, C10-C30 branched alkane, C10-C30 cycloalkane.
Preferably, the vegetable oil is one or more of peanut blend oil, rapeseed blend oil and soybean oil.
The preparation method of the thixotrope solution comprises the following steps:
(1) Weighing the following raw materials in percentage by weight: aluminum stearate, vegetable oil and oil anti-aging agent T501;
(2) Mixing aluminum stearate, vegetable oil and oil product anti-aging agent T501, stirring and ultrasonically dispersing for 5-10min to ensure that the aluminum stearate is uniformly dispersed in the vegetable oil and no obvious agglomeration large particles exist;
(3) Placing the solution obtained in the step (2) under a high-speed emulsifying and dispersing machine for high-speed emulsifying and dispersing for 5-10min, so as to ensure that aluminum stearate is uniformly dispersed;
(4) Heating and stirring the solution obtained in the step (3) in a heating device at 160-180 ℃ for 2-8 hours to ensure that aluminum stearate is uniformly dispersed in vegetable oil and completely dissolved;
(5) Naturally cooling to room temperature to obtain a thixotrope solution, and standing for later use.
The preparation method of the diamond cutting fluid for the silicon carbide wafer comprises the following steps:
(1) Diamond powder is selected as fine micro powder which is finely classified and screened to remove large particles;
(2) Weighing the dispersing agent, the surfactant, the thixotrope solution and the base oil according to the required mass, stirring and ultrasonically mixing uniformly;
(3) Dispersing the solution obtained in the step (2) under a high-speed shearing emulsifying dispersant for 15-30min;
(4) Stirring the solution obtained in the step (3) and simultaneously placing the solution in ultrasonic waves for ultrasonic treatment, and in this state, putting the solution into a container
(1) The diamond powder is added into the system according to the proportion for stirring and ultrasonic dispersion for 15-30min, so that the diamond powder is ensured to be uniformly dispersed in the system and no agglomerated particles exist.
A method for evaluating the suspension stability of a diamond cutting fluid for a silicon carbide wafer comprises the following steps:
(1) Preparing diamond cutting fluid for a silicon carbide wafer to be tested;
(2) Detecting the viscosity of the diamond cutting fluid for the silicon carbide wafer, wherein the rotating speed at least comprises 0.3, 0.6, 1.5, 3 and 6;
(3) Calculating a yield value, wherein the yield value is calculated according to the following formula: (V0.3-V1.5)/100, wherein V0.3 is a viscosity of the diamond cutting fluid for silicon carbide wafer measured at a rotation speed of 0.3r/min, and V1.5 is a viscosity of the diamond cutting fluid for silicon carbide wafer measured at a rotation speed of 1.5 r/min;
(4) The yield value is higher than 40, and the suspension stability of the diamond cutting liquid for the silicon carbide wafer is excellent; the higher the yield value of the diamond cutting fluid for the silicon carbide wafer is, the better the suspension stability is.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following advantages:
The diamond cutting fluid for the silicon carbide wafer solves the problems of poor adhesion performance and poor suspension to abrasive materials of the conventional easy-to-clean suspension fluid, and solves the problems of high viscosity, reduced circulating grinding number and poor cleaning performance of the later-stage waste liquid of the cutting fluid with good suspension property;
The diamond cutting fluid for the silicon carbide wafer reduces the discharge amount of waste liquid and the processing cost while increasing the number of circulating cutting mills;
3. The diamond cutting fluid for the silicon carbide wafer has simple production mode and is easy to produce in mass;
4. the method for judging the suspension stability of the diamond cutting fluid for the silicon carbide wafer is simple to operate, and the research and development time of a formula can be greatly shortened.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below in connection with the embodiments of the present invention. It will be apparent that the described embodiments are some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The diamond cutting fluid for multi-line cutting of the silicon carbide wafer is prepared from the following raw materials in parts by weight:
the thixotrope solution is prepared from the following raw materials in parts by weight:
① Thixotrope solution: weighing the required raw materials according to the proportion, mixing and stirring the goldfish peanut blend oil, aluminum stearate and an oil product anti-aging agent T501 uniformly, emulsifying and dispersing for 5min under a high-speed emulsifying and dispersing machine, heating and stirring the solution in a heating device at 165 ℃ for 4h, ensuring that the aluminum stearate in a container is completely dissolved and dispersed in the goldfish peanut blend oil, and cooling to room temperature for standby.
② Diamond cutting liquid for silicon carbide wafer multi-line cutting: the method comprises the steps of weighing required raw materials except the diamond powder according to the proportion, uniformly mixing and stirring the raw materials, placing the raw materials under a high-speed emulsifying and dispersing machine for high-speed shearing and dispersing for 30min to ensure that the system is uniformly mixed without heterogeneous phase, placing the raw materials into an ultrasonic stirrer for stirring ultrasonic, weighing the diamond powder with required quality, adding the diamond powder into the solution for stirring ultrasonic dispersing for 20min, and ensuring that the diamond powder is completely and uniformly dispersed in the system.
Example 2
The diamond cutting fluid for multi-line cutting of the silicon carbide wafer is prepared from the following raw materials in parts by weight:
67% of C14-C19 isoparaffin;
The thixotrope solution is prepared from the following raw materials in parts by weight: soybean oil 91%
8% Of aluminum stearate
And the oil anti-aging agent T501 percent.
The production steps are as follows:
① Thixotrope solution: the preparation method comprises the steps of weighing required raw materials according to the proportion, mixing and stirring soybean oil, aluminum stearate and an oil product anti-aging agent T501 uniformly, placing under a high-speed emulsifying and dispersing machine for emulsifying and dispersing for 5min, placing the solution in a heating device at 180 ℃ for heating and stirring for 6h, ensuring that the aluminum stearate in a container is completely dissolved and dispersed in the soybean oil, and cooling to room temperature for standby. ② Diamond cutting liquid for silicon carbide wafer multi-line cutting: the method comprises the steps of weighing required raw materials except the diamond powder according to the proportion, uniformly mixing and stirring the raw materials, placing the raw materials under a high-speed emulsifying and dispersing machine for high-speed shearing and dispersing for 30min to ensure that the system is uniformly mixed without heterogeneous phase, placing the raw materials into an ultrasonic stirrer for stirring ultrasonic, weighing the diamond powder with required quality, adding the diamond powder into the solution for stirring ultrasonic dispersing for 20min, and ensuring that the diamond powder is completely and uniformly dispersed in the system.
Comparative example 1
The diamond cutting fluid for multi-line cutting of the silicon carbide wafer is prepared from the following raw materials in parts by weight:
① Weighing the required raw materials, and uniformly mixing and stirring oleyl alcohol polyoxyethylene (3) ether, DISPERBYK-180 and C11-C17 linear alkane;
② Adding diamond powder into the mixed solution obtained by ①, simultaneously placing the ① solution device into ultrasonic waves, and simultaneously carrying out ultrasonic stirring and dispersing for 20min.
Comparative example 2
The diamond cutting fluid for multi-line cutting of the silicon carbide wafer is prepared from the following raw materials in parts by weight:
② Placing the C14-C19 isoparaffin weighed by ① into a heating device for heating, controlling the temperature at 50 ℃,
③ Adding the weighed organic modified bentonite into the ② solution, and uniformly stirring until no large particles exist;
④ Placing the ③ solution into a high-speed emulsifying and dispersing machine to carry out high-speed emulsifying and dispersing for 20min;
⑤ Naturally cooling the ④ solution to room temperature;
⑥ And adding the weighed diamond powder into the ⑤ solution, simultaneously opening a stirring and ultrasonic device, and stirring and ultrasonic for 30min until the abrasive is completely dispersed in the system.
Example 3
A method for evaluating the suspension stability of a diamond cutting fluid for a silicon carbide wafer comprises the following steps:
(1) Preparing diamond cutting fluid for a silicon carbide wafer to be tested;
(2) Detecting the viscosity of the diamond cutting fluid for the silicon carbide wafer by using NDJ-8S (Shanghai Fang Rui instrument limited company), wherein the rotating speed at least comprises 0.3, 0.6, 1.5, 3 and 6;
(3) Calculating a yield value, wherein the yield value is calculated according to the following formula: (V0.3-V1.5)/100, wherein V0.3 is the viscosity of the diamond cutting fluid for silicon carbide wafer measured at a rotational speed of 0.3r/min, and can be regarded as the viscosity of the solution which can be accurately detected at a rotational speed of 0r/min or more and is closest to the stationary state, V1.5 is the viscosity of the diamond cutting fluid for silicon carbide wafer measured at a rotational speed of 1.5r/min, and can be regarded as the viscosity of the solution in a state where the flow of the solution is just started, and the yield value is expressed as the force required for the flow of the fluid just started;
(4) The yield value is higher than 40, and the suspension stability of the diamond cutting liquid for the silicon carbide wafer is excellent; the higher the yield value of the diamond cutting fluid for the silicon carbide wafer is, the better the suspension stability is.
When the suspension stability of the diamond cutting fluid for the silicon carbide wafer is tested by using the method for evaluating the suspension stability of the diamond cutting fluid for the silicon carbide wafer, the suspension stability of the sample with high yield value to the abrasive is better by calculating and comparing the yield value of each sample to be tested.
The evaluation method greatly saves time compared with the traditional method (judging the suspension stability of the diamond cutting fluid through long-time standing).
Test examples
The following tests were performed on the diamond cutting fluids for silicon carbide wafers described in examples 1 and 2 and comparative examples 1 and 2, respectively;
(1) The viscosity V6 is detected by NDJ-8S (Shanghai Fang Rui instruments Co., ltd.), wherein V6 is the viscosity of the diamond cutting fluid for silicon carbide wafer measured at a rotation speed of 6 r/min;
(2) Yield value was determined as described in example 3;
(3) Standing for two weeks, and observing and recording the suspension stability state during standing;
(4) And carrying out multi-wire cutting on silicon carbide by matching with a multi-wire cutting machine, and collecting an application feedback result.
The above data are plotted as table 1;
The results show that ① example 1 and example 2 have the best suspension stability to the abrasive and the corresponding yield value is higher; comparative example 2 times, comparative example 1 was worst and had the smallest yield value, i.e., the magnitude of the yield value was such as to verify the suspension stability of the cutting fluid formulation to abrasive materials; ② As can be seen by comparing example 1 with comparative example 1, the cutting fluid with excellent suspension stability of the abrasive material of the cutting fluid has higher cutting efficiency and better wafer quality; ③ Comparison of the embodiment 2 and the comparative example 2 shows that under the condition of slightly different suspension stability of the cutting fluid, the cutting fluid has more processing grinding numbers, namely the cutting fluid with the same dosage has more cutting times, thus greatly reducing the dosage of the cutting fluid and the discharge amount of the waste liquid in the later period, reducing the production cost and reducing the environmental pollution; the cutting fluid disclosed by the invention has the advantages that the defect of quick heating in the cutting process is overcome, and the cutting fluid is easier to clean in the later period.
While the invention has been described in connection with certain embodiments, it is not intended that the invention be limited thereto; for those skilled in the art to which the present invention pertains and the related art, on the premise of based on the technical scheme of the present invention, the expansion, the operation method and the data replacement should all fall within the protection scope of the present invention.

Claims (6)

1. The diamond cutting fluid for the silicon carbide wafer is characterized by comprising the following raw materials in percentage by weight:
8-20% of diamond powder
0.5 To 2.5 percent of dispersing agent
2-6% Of surfactant
10-40% Of thixotrope solution
31.5 To 79.5 percent of base oil;
wherein, the thixotrope solution comprises the following raw materials:
85-97% of vegetable oil
Aluminum stearate 2-10%
1-5% Of oil anti-aging agent T501;
the surfactant is one or more of tallow amine polyoxyethylene (5) ether, oleyl alcohol polyoxyethylene ether, dodecyl alcohol polyoxyethylene (3) ether, oleyl amine polyoxyethylene (2) ether and oleic acid triglyceride;
The preparation method of the thixotrope solution comprises the following steps:
(1) Weighing the following raw materials in percentage by weight: aluminum stearate, vegetable oil and oil anti-aging agent T501;
(2) Mixing aluminum stearate, vegetable oil and oil product anti-aging agent T501, stirring and ultrasonically dispersing for 5-10min to ensure that the aluminum stearate is uniformly dispersed in the vegetable oil and no obvious agglomeration large particles exist;
(3) Placing the solution obtained in the step (2) under a high-speed emulsifying and dispersing machine for high-speed emulsifying and dispersing for 5-10min, so as to ensure that aluminum stearate is uniformly dispersed;
(4) Heating and stirring the solution obtained in the step (3) in a heating device at 160-180 ℃ for 2-8 hours to ensure that aluminum stearate is uniformly dispersed in vegetable oil and completely dissolved;
(5) Naturally cooling to room temperature to obtain a thixotrope solution, and standing for later use.
2. The diamond cutting fluid for silicon carbide wafers according to claim 1, wherein the diamond powder comprises one or more of single crystal diamond, polycrystalline diamond, and granular diamond, and has an average particle diameter of 0.5 to 40um.
3. The diamond cutting fluid for silicon carbide wafers according to claim 1, wherein the dispersant is one or more of DISPERBYK-2157, DISPERBYK-180, DISPERBYK-110, DISPERBYK-P104S.
4. The diamond cutting fluid for silicon carbide wafers according to claim 1, wherein the base oil is one or more of C10-C30 linear alkanes, C10-C30 branched alkanes, and C10-C30 cycloalkanes.
5. The diamond cutting fluid for silicon carbide wafers according to claim 1, wherein the vegetable oil is one or more of peanut blend oil, rapeseed blend oil and soybean oil.
6. A method for preparing a diamond cutting fluid for silicon carbide wafers according to any one of claims 1 to 5, comprising the steps of:
(1) Diamond powder is selected as fine micro powder which is finely classified and screened to remove large particles;
(2) Weighing the dispersing agent, the surfactant, the thixotrope solution and the base oil according to the required mass, stirring and ultrasonically mixing uniformly;
(3) Dispersing the solution obtained in the step (2) under a high-speed shearing emulsifying dispersing machine for 15-30min;
(4) Stirring the solution obtained in the step (3) and simultaneously placing the solution in ultrasonic waves for ultrasonic treatment, and adding the diamond powder in the step (1) into a system in proportion under the condition of stirring and ultrasonic dispersion for 15-30min to ensure that the diamond powder is uniformly dispersed in the system and has no agglomerated particles.
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Citations (2)

* Cited by examiner, † Cited by third party
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